Guanidine Hydrochloride → HCID 178486745、化合物

HRID 228977ノート

反応式

HRID 228977 の反応式
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:15]=[C:14]2[C:9]([C:10]([O:16][C:17]3[C:18]([CH3:27])=[N:19][C:20]4[C:25]([CH:26]=3)=[CH:24][CH:23]=[CH:22][CH:21]=4)=[CH:11][CH:12]=[N:13]2)=[CH:8][C:7]=1[O:28][CH3:29].C(=O)([O-])[O-].[K+].[K+].Cl.[NH2:37][C:38]([NH2:40])=[NH:39].[H-].[Na+]>O.CN(C)C=O>[CH3:29][O:28][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:6]=1[O:5][CH2:4][CH2:3][CH2:2][NH:39][C:38]([NH2:40])=[NH:37])[N:13]=[CH:12][CH:11]=[C:10]2[O:16][C:17]1[C:18]([CH3:27])=[N:19][C:20]2[C:25]([CH:26]=1)=[CH:24][CH:23]=[CH:22][CH:21]=2

参加物

7

反応物 4

HCID 5742Guanidine HydrochlorideHCID 11430Potassium CarbonateHCID 24758Sodium hydrideHCID 230785037-(3-Chloro-propoxy)-6-methoxy-4-(2-methyl-quinolin-3-yloxy)-quinoline2 回

生成物 1

HCID 178486745HCID 178486745、化合物収率 17%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

N,N-Dimethylformamide (1 ml) was added to 7-(3-chloro-propoxy)-6-methoxy-4-(2-methyl-quinolin-3-yloxy)-quinoline (compound 375) (40 mg), potassium carbonate (41 mg), and guanidine hydrochloride (28 mg). Sodium hydride (39 mg) was added to the mixture, and the mixture was stirred at room temperature overnight. Water was added to the reaction solution, and the mixture was extracted with n-butanol. The n-butanol layer was washed with water and was then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give the title compound (7 mg, yield 17%).

後処理

  1. extractionthe mixture was extracted with n-butanol
  2. washThe n-butanol layer was washed with water
  3. dry with materialwas then dried over anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation under the reduced pressure
  5. customthe residue was purified by thin layer chromatography

出典と根拠

ORDレコード
ord-0aeb4c446e4b458e8d067c1e0b1cde6d
出典データセット
uspto-grants-2009_07
特許番号
US07560558B2

反応ノート

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